分散固相萃取-液相色谱法测定焙烤食品中富马酸二甲酯的含量  

Determination of dimethyl fumarate in bakery food by d-SPE-HPLC-PDA

作　　者：杨杰[1] 罗梦甜 冯迪[2] 苗虹[1] 宋书锋[1] 赵云峰[1] 

机构地区：[1]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京100021 [2]北京工业大学生命科学学院

出　　处：《卫生研究》2015年第3期431-434,439,共5页Journal of Hygiene Research

基　　金：国家质量监督检验检疫总局公益性行业科研专项项目(No.2012104003)

摘　　要：目的建立一种简便快速的分散固相萃取前处理方法 ,结合液相色谱法测定焙烤食品中的富马酸二甲酯。方法样品用甲醇超声提取,采用高速冷冻离心和分散固相萃取净化方式去除油脂、色素等杂质,采用C18柱（4.6 mm×25 mm,5μm）,流动相为甲醇-0.03 mol/L乙酸钠和0.008 mol/L溴化四丁基铵溶液,检测波长220nm。结果该方法在0.1-20μg/ml范围内呈良好线性,r〉0.999,在不同空白基质样品中不同添加水平下,平均回收率为82.8%-107.5%,相对标准偏差（RSD）为3.30%-7.30%（n=6）,检出限（LOD）为0.4 mg/kg,定量限（LOQ）为1.0 mg/kg。结论该方法简便、快速、准确,适用于焙烤食品中富马酸二甲酯含量的检测。Objective To establish a simple and rapid pretreatment method with dispersive solid phase extraction （d-SPE） by HPLC for determination of dimethyl fumarate in bakery foods. Methods Dimethyl fumarate in samples was ultrasonically extracted by methanol, and cleaned up with d-SPE. Then, it was separated on Clschromatographic column （4.6 mm×25 mm,5μm） with a mixture of methanol - 0.03 mol/L sodium acetate and 0. 008 mol/L tetrabutyl ammonium bromide （40： 60, V/V） as mobile phase. The photodiode array detector was used in the determination under λ = 220 nm. Results In the linear range of 0. 1 - 25 μg/ml,the correlation coefficients was r 〉 0. 999, and the average recoveries of the spiked samples were in the range of 82.8% - 107.5 % with relative standard deviations（RSD）in the range of 3.30% -7.30% （n = 6 ）. The limit of detection （LOD） was 0.4 mg/kg, and the limit of quantification was 1.0 mg/kg. Conclusion The method is simple, rapid, sensitive and accurate, and suitable for determine dimethyl fumarate in bakery foods.

关 键 词：分散固相萃取 富马酸二甲酯 液相色谱法 焙烤食品 

分 类 号：R155.5[医药卫生—营养与食品卫生学] TS207.3[医药卫生—公共卫生与预防医学]